CN116639706A - Process for producing electronic chemical ammonia water - Google Patents
Process for producing electronic chemical ammonia water Download PDFInfo
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- CN116639706A CN116639706A CN202310760088.6A CN202310760088A CN116639706A CN 116639706 A CN116639706 A CN 116639706A CN 202310760088 A CN202310760088 A CN 202310760088A CN 116639706 A CN116639706 A CN 116639706A
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- ammonia water
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- ammonia
- following
- purifying
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 235000011114 ammonium hydroxide Nutrition 0.000 title claims abstract description 48
- 239000000126 substance Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims description 30
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000012528 membrane Substances 0.000 claims abstract description 31
- 238000001704 evaporation Methods 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 7
- -1 polyoxyethylene Polymers 0.000 claims description 32
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 239000002131 composite material Substances 0.000 claims description 17
- 229910021389 graphene Inorganic materials 0.000 claims description 17
- ZBSKZKPSSKTLNE-UHFFFAOYSA-N 4-methylpent-3-enoxysilane Chemical compound CC(=CCCO[SiH3])C ZBSKZKPSSKTLNE-UHFFFAOYSA-N 0.000 claims description 16
- 230000008020 evaporation Effects 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229920006197 POE laurate Polymers 0.000 claims description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 10
- 239000000194 fatty acid Substances 0.000 claims description 10
- 229930195729 fatty acid Natural products 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000005507 spraying Methods 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 239000006096 absorbing agent Substances 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 20
- 229910021645 metal ion Inorganic materials 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- JEWCZPTVOYXPGG-UHFFFAOYSA-N ethenyl-ethoxy-dimethylsilane Chemical compound CCO[Si](C)(C)C=C JEWCZPTVOYXPGG-UHFFFAOYSA-N 0.000 description 2
- 229940070765 laurate Drugs 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000000998 batch distillation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/024—Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
- B01D1/305—Demister (vapour-liquid separation)
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The application relates to the technical field of ammonia water production, and particularly discloses an electronic chemical ammonia water production process. An electronic chemical ammonia water production process comprises the following steps: and (3) deoiling and purifying liquid ammonia, evaporating at low temperature, adsorbing, filtering, cooling, primary mixing and absorbing, gas stripping, secondary mixing and absorbing, cooling, purifying by a filter membrane and preparing to obtain the electronic chemical ammonia water. In the application, oily impurities in the liquid ammonia are removed by deoiling and purifying, then impurities such as metal ions, TOC and the like in raw materials are removed by evaporating and adsorbing at low temperature, and then particles and other impurities are removed by a series of operations such as filtering, gas stripping, filter membrane purifying and the like, so that the purity of the prepared ammonia water is improved.
Description
Technical Field
The application relates to the technical field of ammonia water production, in particular to an electronic chemical ammonia water production process.
Background
With the rapid development of the semiconductor industry in China, the demand for high-purity electronic chemicals has increased dramatically. The high-purity electronic grade ammonia water plays an important role in the manufacturing industries of integrated circuits, LCD (liquid crystal display) and the like, and particles and partial metal impurities on the surfaces of activated silicon wafers and particles can be removed by utilizing the weak alkalinity of the ammonia water. Common ammonia production processes include batch distillation, membrane filtration and absorption, resin filtration, etc., but the ammonia produced by these processes is not pure enough and is difficult to use in the field of electronic chemistry.
Disclosure of Invention
In order to improve the purity of the prepared ammonia water, the application provides a production process of electronic chemical ammonia water.
The application provides a production process of electronic chemical ammonia water, which adopts the following technical scheme:
an electronic chemical ammonia water production process comprises the following steps:
and (3) deoiling and purifying liquid ammonia, evaporating at low temperature, adsorbing, filtering, cooling, primary mixing and absorbing, gas stripping, secondary mixing and absorbing, cooling, purifying by a filter membrane and preparing to obtain the electronic chemical ammonia water.
By adopting the technical scheme, oily impurities in the liquid ammonia are removed by deoiling and purifying, then impurities such as metal ions and TOC in raw materials are removed by evaporating and adsorbing at low temperature, and then particles and other impurities are removed by a series of operations such as filtering, gas stripping, filter membrane purifying and the like, so that the purity of the prepared ammonia water is improved.
In a specific embodiment, the liquid ammonia is pretreated before deoiling and purifying, and a treating agent is added to the liquid ammonia, wherein the treating agent comprises a mixture of polyoxyethylene fatty acid ester and polyoxyethylene laurate.
Through adopting above-mentioned technical scheme, polyoxyethylene fatty acid ester and laurate polyoxyethylene ester can be dissolved in the oily impurity in the liquid ammonia, separates out ammonia water, and laurate polyoxyethylene ester can also promote the dispersion of treating agent to make the oily impurity in the liquid ammonia can better separation, convenient deoiling purification.
In a specific embodiment, the weight ratio of the treating agent to the liquid ammonia is 1: (150-250).
By adopting the technical scheme, the application further limits the ratio of the treating agent to the liquid ammonia, thereby improving the purification effect of deoiling and purifying.
In a specific implementation manner, in the deoiling and purifying step, deoiling and purifying are performed by using an oil-water separator, wherein a graphene composite membrane is arranged in the oil-water separator; the preparation method of the graphene composite membrane comprises the following steps:
uniformly stirring and mixing dimethylvinylethoxysilane, ethanol and water to obtain a spraying liquid; stirring the graphite oxide powder, spraying the spraying liquid on the graphite oxide powder in the stirring process, and drying to obtain modified powder;
adding the modified powder into water, stirring uniformly to obtain a dispersion liquid, filtering the dispersion liquid by using a microporous filter membrane, loading the modified powder on the microporous filter membrane, and carrying out vacuum drying to obtain the graphene composite membrane.
By adopting the technical scheme, the dimethylvinylethoxysilane is firstly dissolved in ethanol and then sprayed on the surface of the graphite oxide powder, and then the surface of the graphite oxide powder is dried, so that the dimethylvinylethoxysilane coats the graphite oxide powder to finish the modification of the graphite oxide powder, and the graphite oxide powder is uniformly loaded on a microporous filter membrane to obtain a graphene composite membrane; the addition of the graphite oxide powder can improve the purification effect of deoiling and purifying; in addition, the graphite oxide powder has a better adsorption effect, so that the raw materials can be further purified, and the purity of the prepared ammonia water is further improved.
In a specific embodiment, the weight ratio of the dimethylvinylethoxysilane to the graphite oxide powder is 1: (65-75).
By adopting the technical scheme, the application further limits the proportion of the dimethylvinylethoxysilane to the graphite oxide powder, so that the dimethylvinylethoxysilane can better coat the graphite oxide powder, and the modification effect on the graphite oxide powder is improved.
In a specific embodiment, in the low-temperature evaporation step, low-temperature evaporation is performed by using a liquid ammonia evaporation device; the liquid ammonia evaporation equipment comprises a barrel and an electric heating element arranged on the barrel, a feed inlet is formed in the bottom wall of the barrel, a discharge pipe is arranged on the top wall of the barrel, and a demister is arranged on the discharge pipe.
By adopting the technical scheme, impurities such as metal ions, TOC and the like in the raw materials can be effectively removed by utilizing the liquid ammonia evaporation equipment.
In a specific embodiment, the temperature in the low temperature evaporation step is 20-30 ℃.
In a specific embodiment, the primary and secondary mixing absorption steps are each performed using a microchannel mixing absorber.
In a specific embodiment, in the stripping step, stripping is performed using a stripping column.
In a specific embodiment, the filtration step is performed by 10nm microchannel filtration.
In summary, the present application includes at least one of the following beneficial technical effects:
1. according to the method, oily impurities in the liquid ammonia are removed by deoiling and purifying, then impurities such as metal ions and TOC in raw materials are removed by evaporating and adsorbing at low temperature, and then particles and other impurities are removed by a series of operations such as filtering, gas stripping and filter membrane purifying, so that the purity of the prepared ammonia water is improved;
2. according to the method, the liquid ammonia is pretreated by the treating agent, the polyoxyethylene fatty acid ester and the polyoxyethylene laurate in the treating agent can be dissolved in oily impurities in the liquid ammonia to separate ammonia water, and the polyoxyethylene laurate can also promote the dispersion of the treating agent, so that the oily impurities in the liquid ammonia can be better separated, and the deoiling and purifying are convenient;
3. according to the preparation method, dimethyl vinyl ethoxy silane is firstly dissolved in ethanol and then sprayed on the surface of graphite oxide powder, and then the graphite oxide powder is coated by the dimethyl vinyl ethoxy silane, so that the modification of the graphite oxide powder is completed, and the graphite oxide powder is uniformly loaded on a microporous filter membrane to obtain a graphene composite membrane; the addition of the graphite oxide powder can improve the purification effect of deoiling and purifying; in addition, the graphite oxide powder has a better adsorption effect, so that the raw materials can be further purified, and the purity of the prepared ammonia water is further improved.
Drawings
FIG. 1 is a schematic view showing the overall structure of a liquid ammonia evaporation apparatus according to example 1 of the present application.
Reference numerals illustrate: 1. a cylinder; 2. an electric heating element; 3. a feed inlet; 4. a discharge pipe; 5. and a demister.
Detailed Description
The present application will be described in further detail with reference to examples.
All the starting materials in the examples are commercially available.
Preparation example
Preparation example 1
Preparation example 1 provides a preparation method of a graphene composite membrane, which comprises the following steps:
uniformly stirring and mixing dimethylvinylethoxysilane, ethanol and water to obtain a spraying liquid; adding graphite oxide powder into a high-speed mixer, spraying liquid on the graphite oxide powder in the stirring process, stirring for 0.5h after spraying, and drying at 50 ℃ for 2h to obtain modified powder; wherein the weight ratio of the dimethylvinylethoxysilane, the ethanol and the water in the spraying liquid is 5:18:2; the weight ratio of the dimethylvinylethoxysilane to the graphite oxide powder is 1:60;
adding the modified powder into water, stirring uniformly to obtain a dispersion liquid, filtering the dispersion liquid by using a microporous filter membrane to load the modified powder on the microporous filter membrane, and vacuum drying at 30 ℃ for 24 hours to obtain a graphene composite membrane; wherein the weight ratio of the modified powder to the water in the dispersion is 1:5.
preparation example 2
Preparation example 2 differs from preparation example 1 in that the weight ratio of dimethylvinylethoxysilane to graphite oxide powder is 1: 65. The remaining steps are identical to those of preparation 1.
Preparation example 3
Preparation example 3 differs from preparation example 1 in that the weight ratio of dimethylvinylethoxysilane to graphite oxide powder is 1:70; the remaining steps are identical to those of preparation 1.
Preparation example 4
Preparation example 4 differs from preparation example 1 in that the weight ratio of dimethylvinylethoxysilane to graphite oxide powder is 1:75; the remaining steps are identical to those of preparation 1.
Preparation example 5
Preparation example 5 differs from preparation example 1 in that the weight ratio of dimethylvinylethoxysilane to graphite oxide powder is 1:80; the remaining steps are identical to those of preparation 1.
Examples
Example 1
Example 1 provides a liquid ammonia vaporization apparatus.
Referring to fig. 1, a liquid ammonia evaporation device comprises a barrel 1, wherein an electric heating element 2 is arranged on the barrel 1, a feed inlet 3 is formed in the bottom wall of the barrel 1, a discharge pipe 4 is communicated with the top wall of the barrel 1, and a demister 5 is arranged on the discharge pipe 4.
Example 1 also provides a process for producing an aqueous ammonia solution for electronic chemicals, comprising the steps of:
adding liquid ammonia into an oil-water separator for deoiling and purifying, wherein the graphene composite membrane in the oil-water separator is the graphene composite membrane in preparation example 1; then, the deoiled and purified liquid ammonia enters the cylinder 1 through the feed inlet 3 to be evaporated at a low temperature of 20 ℃ to obtain ammonia gas, the ammonia gas is adsorbed by a high-purity Teflon material, and then is filtered by a 10nm microchannel and cooled by a cooler; adding the cooled ammonia gas into a micro-channel mixing absorber, adding ultrapure water at the same time to perform primary mixing absorption, and then performing gas stripping by using a gas stripping tower; adding the ammonia gas after stripping into the micro-channel mixing absorber again, adding ultrapure water to perform secondary mixing absorption, and then cooling by using a cooler; and finally purifying by using a nanofiltration membrane, and blending by using ultrapure water to obtain the electronic chemical ammonia water.
Examples 2 to 5
As shown in table 1, the main difference between examples 2 to 5 and example 1 is the different choice of graphene composite membrane.
Table 1 selection of graphene composite films in examples 2-5
| Sample of | Selection of graphene composite membrane |
| Example 1 | Preparation example 1 |
| Example 2 | Preparation example 2 |
| Example 3 | Preparation example 3 |
| Example 4 | Preparation example 4 |
| Example 5 | Preparation example 5 |
Example 6
Example 6 differs from example 3 in that a treating agent is added to the liquid ammonia and stirred uniformly to obtain treated liquid ammonia; adding the treated liquid ammonia into an oil-water separator for deoiling and purifying; wherein the treating agent comprises a mixture of polyoxyethylene fatty acid ester and polyoxyethylene laurate, and the weight ratio of the polyoxyethylene fatty acid ester to the polyoxyethylene laurate is 2:1, a step of; the weight ratio of the treating agent to the liquid ammonia is 1:100; the remaining steps are in accordance with example 3.
Example 7
Example 7 differs from example 6 in that the weight ratio of treating agent to liquid ammonia is 1:150; the remaining steps are in accordance with example 6.
Example 8
Example 8 differs from example 6 in that the weight ratio of treating agent to liquid ammonia is 1:200; the remaining steps are in accordance with example 6.
Example 9
Example 9 differs from example 6 in that the weight ratio of treating agent to liquid ammonia is 1:250; the remaining steps are in accordance with example 6.
Example 10
Example 10 differs from example 6 in that the weight ratio of treating agent to liquid ammonia is 1:300; the remaining steps are in accordance with example 6.
Example 11
Example 11 differs from example 8 in that the treating agent is a polyoxyethylene fatty acid ester; the remaining steps are in accordance with example 8.
Example 12
Example 12 differs from example 8 in that the treating agent is polyoxyethylene laurate; the remaining steps are in accordance with example 8.
Example 13
Example 13 differs from example 8 in that the deoiled and purified liquid ammonia is fed into the cylinder 1 through the feed port 3 and evaporated at a low temperature of 25 ℃ to obtain ammonia gas; the remaining steps are in accordance with example 8.
Example 14
Example 14 differs from example 8 in that the deoiled and purified liquid ammonia is fed into the cylinder 1 through the feed port 3 and evaporated at a low temperature of 30 ℃ to obtain ammonia gas; the remaining steps are in accordance with example 8.
Comparative example
Comparative example 1
The intermittent distillation method is used for preparing the electronic chemical ammonia water.
Performance test purity detection: the electronic chemicals ammonia water in each example and comparative example is detected to obtain the content of metal ions and anions in the ammonia water, and the lower the content of the metal ions and anions is, the higher the purity of sulfuric acid is; the metal ion is exemplified by sodium ion; anions are exemplified by chloride ions.
TABLE 2 Performance test results of electronic chemical Ammonia
| Sample of | Metal ion (ppt) | Anions (ppb) |
| Example 1 | ＜10 | ＜10 |
| Example 2 | ＜8 | ＜8 |
| Example 3 | ＜8 | ＜7 |
| Example 4 | ＜8 | ＜8 |
| Example 5 | ＜10 | ＜10 |
| Example 6 | ＜6 | ＜6 |
| Example 7 | ＜4 | ＜5 |
| Example 8 | ＜4 | ＜5 |
| Example 9 | ＜4 | ＜5 |
| Example 10 | ＜6 | ＜6 |
| Example 11 | ＜10 | ＜10 |
| Example 12 | ＜9 | ＜9 |
| Example 13 | ＜3 | ＜4 |
| Example 14 | ＜3 | ＜3 |
| Comparative example 1 | ＜50 | ＜45 |
In combination with example 1 and comparative example 1, the electronic chemical ammonia water in example 1 has higher purity, and it can be seen that by using the process for producing electronic chemical ammonia water in the present application, oily impurities in liquid ammonia are removed by deoiling and purifying, then evaporating at low temperature, removing impurities such as metal ions and TOC in raw materials, then removing particles and other impurities through a series of operations such as filtration, gas stripping, filter membrane purification, etc., thereby improving the purity of the produced ammonia water.
In combination with examples 1 to 5, the electronic chemicals ammonia water in examples 2 to 4 had a higher purity, and it can be seen that the ratio of dimethylvinylethoxysilane to graphite oxide powder in the preparation of the graphene composite film was preferably 1: (65-75), the separation effect of the prepared graphene composite membrane is good, and the purity of ammonia water is improved.
In combination with example 3 and example 6, the electronic chemical ammonia water in example 6 has higher purity, and the fact that the mixture composed of polyoxyethylene fatty acid ester and polyoxyethylene laurate is utilized to pretreat the liquid ammonia before deoiling and purifying the liquid ammonia can separate the ammonia water in oily impurities, so that deoiling and purifying are convenient.
In combination with examples 6 and examples 7 to 10, the electronic chemical ammonia in examples 7 to 9 is higher in purity, and it can be seen that when the pretreatment agent is used to pretreat liquid ammonia, the ratio of the treatment agent to liquid ammonia is preferably 1: (150-250), the treatment effect on liquid ammonia is better.
In combination of examples 8, 11 and 12, the electronic chemical ammonia water of example 8 has the highest purity, and it is found that when the liquid ammonia is pretreated with the treating agent, the treating agent is preferably a mixture of polyoxyethylene fatty acid ester and polyoxyethylene laurate, and the polyoxyethylene laurate can promote dispersion of the polyoxyethylene fatty acid ester, so that oily impurities in the liquid ammonia can be better separated, and thus the purity of the prepared ammonia water is improved.
In combination with examples 8, 13 and 14, it was found that the purity of the produced ammonia water can be improved by increasing the evaporation temperature at a temperature of 20 to 30℃when evaporation is performed using a liquid ammonia evaporation apparatus.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. The production process of the electronic chemical ammonia water is characterized by comprising the following steps of: the method comprises the following steps:
and (3) deoiling and purifying liquid ammonia, evaporating at low temperature, adsorbing, filtering, cooling, primary mixing and absorbing, gas stripping, secondary mixing and absorbing, cooling, purifying by a filter membrane and preparing to obtain the electronic chemical ammonia water.
2. The process for producing the ammonia water for electronic chemicals according to claim 1, wherein the process comprises the following steps: pretreatment is carried out before deoiling and purifying liquid ammonia, and a treating agent is added into the liquid ammonia, wherein the treating agent comprises a mixture of polyoxyethylene fatty acid ester and polyoxyethylene laurate.
3. The process for producing the ammonia water for electronic chemicals according to claim 1, wherein the process comprises the following steps: the weight ratio of the treating agent to the liquid ammonia is 1: (150-250).
4. The process for producing the ammonia water for electronic chemicals according to claim 1, wherein the process comprises the following steps: in the deoiling and purifying step, an oil-water separator is utilized for deoiling and purifying, and a graphene composite membrane is arranged in the oil-water separator; the preparation method of the graphene composite membrane comprises the following steps:
uniformly stirring and mixing dimethylvinylethoxysilane, ethanol and water to obtain a spraying liquid; stirring the graphite oxide powder, spraying the spraying liquid on the graphite oxide powder in the stirring process, and drying to obtain modified powder;
adding the modified powder into water, stirring uniformly to obtain a dispersion liquid, filtering the dispersion liquid by using a microporous filter membrane, loading the modified powder on the microporous filter membrane, and carrying out vacuum drying to obtain the graphene composite membrane.
5. The process for producing the ammonia water for electronic chemicals according to claim 4, wherein the process comprises the following steps: the weight ratio of the dimethylvinylethoxysilane to the graphite oxide powder is 1: (65-75).
6. The process for producing the ammonia water for electronic chemicals according to claim 1, wherein the process comprises the following steps: in the low-temperature evaporation step, low-temperature evaporation is performed by using liquid ammonia evaporation equipment; the liquid ammonia evaporation equipment comprises a barrel body (1) and an electric heating element (2) arranged on the barrel body (1), a feed inlet (3) is formed in the bottom wall of the barrel body (1), a discharge pipe (4) is arranged on the top wall of the barrel body (1), and a demister (5) is arranged on the discharge pipe (4).
7. The process for producing the ammonia water for electronic chemicals according to claim 6, wherein the process comprises the following steps: the temperature in the low-temperature evaporation step is 20-30 ℃.
8. The process for producing the ammonia water for electronic chemicals according to claim 1, wherein the process comprises the following steps: and in the primary mixed absorption and the secondary mixed absorption steps, a microchannel mixed absorber is used for mixed absorption.
9. The process for producing the ammonia water for electronic chemicals according to claim 1, wherein the process comprises the following steps: in the stripping step, a stripping tower is utilized for stripping.
10. The process for producing the ammonia water for electronic chemicals according to claim 1, wherein the process comprises the following steps: in the filtration step, filtration is performed through 10nm microchannels.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310760088.6A CN116639706A (en) | 2023-06-26 | 2023-06-26 | Process for producing electronic chemical ammonia water |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310760088.6A CN116639706A (en) | 2023-06-26 | 2023-06-26 | Process for producing electronic chemical ammonia water |
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| Publication Number | Publication Date |
|---|---|
| CN116639706A true CN116639706A (en) | 2023-08-25 |
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|---|---|---|---|
| CN202310760088.6A Pending CN116639706A (en) | 2023-06-26 | 2023-06-26 | Process for producing electronic chemical ammonia water |
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| Country | Link |
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